Preparation Method of Superhydrophobic / Superoleophilic Polyester Fiber Felt for Oil-Water Emulsion Separation

Abstract

The invention discloses a preparation method of a superhydrophobic / superoleophilic polyester fiber felt for oil-water emulsion separation, which is specifically implemented according to the following steps: Step 1, prepare a superhydrophobic / superoleophilic SiO2-ZrO2 functional slurry; Step 2, deposit the SiO2-ZrO2 functional gel coating obtained in Step 1 on the fiber surface of the polyester fiber felt through spraying treatment; Step 3, further crosslink and cure the SiO2-ZrO2 functional gel coating deposited on the fiber surface of the polyester fiber felt in Step 2 through microwave treatment to obtain a superhydrophobic / superoleophilic polyester fiber felt. The method of the invention solves the problem that existing materials cannot simultaneously meet the requirements of low cost, high efficiency and corrosion resistance.

Description

Technical Field

[0001] The present invention belongs to the technical field of oil-water separation, and relates to a preparation method of a superhydrophobic / superoleophilic polyester fiber felt for separating oil-water emulsions. Background Art

[0002] Emulsions in oily wastewater exist stably in the form of small droplets with a particle size below 20 μm, and are divided into two types: oil-in-water (O / W) and water-in-oil (W / O). Due to the presence of an interfacial film on the droplet surface, traditional static-separation methods cannot be directly used for separation, and demulsification is required first. Currently, the most widely used emulsion separation technology is membrane separation technology, which realizes the separation of oil-water emulsions by regulating the wettability and pore size of the membrane. This technology has a relatively mature process, but the material cost is high and the separation efficiency is low. In addition, the mechanical and corrosion resistance properties of the membrane material are poor, the membrane pores are easily blocked and contaminated during the membrane separation process, and the recyclability is not ideal. Emulsion separation can also be achieved by selectively adsorbing the oil phase from the oil-water emulsion, which has the advantages of simple operation and high separation efficiency. The main adsorption-type oil-water emulsion separation materials include aerogels, porous foams, and sponges, but it is difficult for these materials to simultaneously meet the technical requirements of low cost, high efficiency, and corrosion resistance.

[0003] Polyester fiber felt has a loose porous structure, low cost, and good mechanical properties, and is an ideal raw material for preparing adsorption-type oil-water emulsion separation materials. However, polyester fiber felt does not have selectivity for the adsorption of oil or water. In addition, as a linear polymer, it is extremely easy to swell or degrade in oil / water mixtures. These problems determine that polyester fiber felt cannot be used as a highly corrosion-resistant and reusable adsorption-type oil-water emulsion separation material for engineering applications. Summary of the Invention

[0004] The purpose of the present invention is to provide a preparation method of a superhydrophobic / superoleophilic polyester fiber felt for separating oil-water emulsions, so as to solve the problem that existing materials cannot simultaneously meet the requirements of low cost, high efficiency, and corrosion resistance.

[0005] The technical solution adopted by the present invention is a preparation method of a superhydrophobic / superoleophilic polyester fiber felt for separating oil-water emulsions, which is specifically implemented according to the following steps:

[0006] Step 1, prepare a superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry;

[0007] Step 2, deposit the SiO 2 -ZrO 2 functional gel coating obtained in Step 1 on the fiber surface of the polyester fiber felt by spraying treatment;

[0008] Step 3, deposit the SiO 2-ZrO 2 The functional gel coating is further cross-linked and cured to obtain a superhydrophobic / superoleophilic polyester fiber felt.

[0009] The features of the present invention also lie in that

[0010] The specific process of Step 1 is as follows: at room temperature, zirconium butoxide is added to an organic solvent, and after magnetic stirring for 2 h to 6 h, tetraethyl orthosilicate and a long-chain silane are added in sequence, and stirring is continued for 1 h to 4 h, and then it is left to stand for aging, thus obtaining superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry.

[0011] The concentration of the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry is 0.01 mol / L to 0.2 mol / L, and the mass ratio of zirconium butoxide:tetraethyl orthosilicate:long-chain silane is 1:1 to 4:0.01 to 0.5.

[0012] The organic solvent is one or both of absolute ethanol and absolute methanol, and the long-chain silane is one or several of dodecyltrimethoxysilane, dodecyltriethoxysilane, hexadecyltrimethoxysilane, hexadecyltrimethoxysilane, octadecyltrimethoxysilane, and octadecyltriethoxysilane.

[0013] In Step 2, the process of spraying treatment is as follows: by means of air spraying, the slurry obtained in Step 2 is sprayed onto the surface of the fiber felt, and then the slurry is uniformly coated by repeated extrusion, and finally it is dried in an oven at 30 °C to 80 °C for 5 min to 60 min.

[0014] The spraying amount is based on the fact that the slurry can completely wet the surface and inside of the fiber felt.

[0015] In Step 3, the microwave curing power is 100 W to 1800 W, and the curing time is 1 min to 60 min.

[0016] The beneficial effects of the present invention are

[0017] (1) For the preparation method of the superhydrophobic / superoleophilic polyester fiber felt for oil-water emulsion separation of the present invention, the use of the SiO 2 component not only reduces the coating cost, but also ensures the sufficient immobilization of the long-chain silane modifier; the compounding of the ZrO 2 component further improves the stability and corrosion resistance of the polyester fiber felt. Therefore, the SiO 2 -ZrO 2 composite coating material takes into account both SiO 2 and ZrO 2The advantages of each material endow the polyester fiber felt with the material advantages of low cost and high corrosion resistance, and the coating has good bonding strength.

[0018] (2) The polyester fiber felt prepared by the method of the present invention has superhydrophobic / superoleophilic properties and excellent oil absorption and oil retention performance.

[0019] (3) The polyester fiber felt prepared by the method of the present invention is an adsorption-type oil-water emulsion separation material, which can adsorb the oil phase from the water-in-oil or oil-in-water emulsion system, and has the advantages of good oil-water selectivity and high separation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 is the infrared absorption (FT-IR) spectrum of the superhydrophobic / superoleophilic polyester fiber felt prepared by the method of the present invention;

[0021] Figure 2 is the scanning electron microscope (SEM) photograph of the superhydrophobic / superoleophilic polyester fiber felt prepared by the method of the present invention;

[0022] Figure 3 is the wettability photograph of the superhydrophobic / superoleophilic polyester fiber felt prepared by the method of the present invention for water and oil;

[0023] Figure 4 is the contact angle of the superhydrophobic / superoleophilic polyester fiber felt prepared by the method of the present invention for water and oil;

[0024] Figure 5 is the photograph of the superhydrophobic / superoleophilic polyester fiber felt prepared by the method of the present invention separating an oil-water emulsion;

[0025] Figure 6 is the O / W emulsion photograph of the superhydrophobic / superoleophilic polyester fiber felt prepared by the method of the present invention and the water-in-oil (O / W) oil-water emulsion;

[0026] Figure 7 is Figure 6 the optical micrograph of each emulsion in, where (a) corresponds to the O / W emulsion, (b) corresponds to fiber felt - O / W, (c) corresponds to fiber felt NaCl -O / W, (d) corresponds to fiber felt HCl -O / W, (e) corresponds to fiber felt NaOH -O / W;

[0027] Figure 8 is the W / O emulsion photograph of the superhydrophobic / superoleophilic polyester fiber felt prepared by the method of the present invention and the oil-in-water (W / O) oil-water emulsion treated;

[0028] Figure 9 is Figure 8Optical micrographs of each emulsion, where (a) corresponds to the W / O emulsion, (b) corresponds to the fiber mat-W / O, (c) corresponds to the fiber mat NaCl -W / O, (d) corresponds to the fiber mat HCl -W / O, (e) corresponds to the fiber mat NaOH -W / O. Specific embodiments

[0029] The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0030] The present invention provides a method for preparing a superhydrophobic / superoleophilic polyester fiber mat for oil-water emulsion separation, which is specifically implemented according to the following steps:

[0031] Step 1, prepare a superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry;

[0032] The specific process is as follows: at room temperature, add zirconium butoxide to an organic solvent, and after magnetic stirring for 2 h to 6 h, successively add tetraethyl orthosilicate and a long-chain silane. The mass ratio of zirconium butoxide:tetraethyl orthosilicate:long-chain silane is 1:1 to 4:0.01 to 0.5, continue stirring for 1 h to 4 h, and then stand for aging to obtain the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry. The concentration of the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry is 0.01 mol / L to 0.2 mol / L;

[0033] Among them, the organic solvent is one or two of absolute ethanol and absolute methanol;

[0034] The long-chain silane is one or several of dodecyltrimethoxysilane, dodecyltriethoxysilane, hexadecyltrimethoxysilane, hexadecyltrimethoxysilane, octadecyltrimethoxysilane, and octadecyltriethoxysilane;

[0035] Step 2, using the air spraying method, spray the slurry obtained in step 2 onto the surface of the fiber mat. The spraying amount is such that the slurry can completely wet the surface and interior of the fiber mat. Then, make the slurry evenly coated by repeated extrusion. Finally, dry it in an oven at 30 °C to 80 °C for 5 min to 60 min to deposit the SiO 2 -ZrO 2 functional gel coating obtained in step 1 on the fiber surface of the polyester fiber mat;

[0036] Step 3, through microwave treatment, the SiO 2 -ZrO 2The functional gel coating is further crosslinked and cured with a microwave curing power of 100 W to 1800 W and a curing time of 1 min to 60 min to obtain a superhydrophobic / superoleophilic polyester fiber felt.

[0037] The method of the present invention deposits a layer of SiO 2 -ZrO 2 functional coating on the fiber surface of the polyester fiber felt, endowing the polyester fiber felt with excellent stability and corrosion resistance. At the same time, through the modification of long-chain hydrocarbon groups in the coating, the polyester fiber felt is endowed with excellent superhydrophobic / superoleophilic properties and has a special function of adsorbing and separating the oil-phase components from the oil-water emulsion. Compared with the same type of adsorption-type oil-water emulsion separation materials, it shows the product advantages of low cost, high efficiency and corrosion resistance.

[0038] Example 1

[0039] Step 1, prepare a superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry;

[0040] The specific process is as follows: at room temperature, zirconium butoxide is added to absolute ethanol, and after magnetic stirring for 2 h, tetraethyl orthosilicate and dodecyltrimethoxysilane are added in sequence. The molar ratio of zirconium butoxide:tetraethyl orthosilicate:dodecyltrimethoxysilane is 1:1:0.01, and stirring is continued for 1 h, followed by static aging to obtain a superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry, and the concentration of the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry is 0.01 mol / L;

[0041] Step 2, by means of air spraying, spray the slurry obtained in Step 2 onto the surface of the fiber felt. The spraying amount is such that the slurry can completely wet the surface and inside of the fiber felt. Subsequently, the slurry is evenly coated by repeated extrusion, and finally dried in an oven at 30 °C for 60 min to remove the organic solvent in the gel coating, so as to deposit the SiO 2 -ZrO 2 functional gel coating on the fiber surface of the polyester fiber felt;

[0042] Step 3, further crosslink and cure the SiO 2 -ZrO 2 functional gel coating deposited on the fiber surface of the polyester fiber felt in Step 2 by microwave treatment. The microwave curing power is 100 W and the curing time is 60 min to obtain a superhydrophobic / superoleophilic polyester fiber felt.

[0043] The FT-IR spectrum of the superhydrophobic / superoleophilic polyester fiber felt is as Figure 1As shown, where 3370 cm -1 and 3401 cm -1 characteristic peaks correspond to the absorption peaks of the vibration of -OH groups in the coating; 2917 cm -1 corresponds to the stretching vibration of -CH 2 CH 3 in the long-chain hydrocarbon group modification group; 1589 cm -1 corresponds to the absorption peak of the benzene ring skeleton of the polyester fiber felt; 1468 cm -1 and 1384 cm -1 correspond to the bending vibration of the C-H group of the polyester fiber; 1278 cm -1 and 1018 cm -1 correspond to the stretching vibration of the C-O group; 934 cm -1 corresponds to the absorption peak of the -Si-OH group; 778 cm -1 and 459 cm -1 correspond to the absorption peak of the Si-O-Si group; 637 cm -1 corresponds to the absorption peak of the Zr-O-Zr group; 1100 cm -1 corresponds to the absorption peak of the Si-O-Zr group. Thus, it can be seen that SiO 2 -ZrO 2 composite coating has been successfully coated on the surface of the fibers of the polyester fiber felt.

[0044] As Figure 2 shown, the fiber surface is densely coated with SiO 2 -ZrO 2 composite coating. The surface of the coating is rough, showing a hilly shape. The rough surface can increase the specific surface area of the fibers, which has a positive effect on improving the superhydrophobic / superoleophilic and oil absorption properties of the fiber felt.

[0045] The superhydrophobic / superoleophilic polyester fiber felt has excellent oil absorption and oil retention properties. Its oil absorption rates are: n-hexane 11.8 g / g, gasoline 13.1 g / g, petroleum ether 12.8 g / g, cyclohexane 15.2 g / g, vegetable oil 25.6 g / g, silicone oil 34.8 g / g, chlorobenzene 20.7 g / g, dichloromethane 21.4 g / g, chloroform 22.6 g / g; its oil retention rates are: n-hexane 91.4, gasoline 91.8, petroleum ether 91.5, cyclohexane 92.2, vegetable oil 98.2, silicone oil 99.3, chlorobenzene 93.5, dichloromethane 94.2, chloroform 95.4.

[0046] As Figure 3 shown, water will form spherical water droplets on the surface of the fiber felt. After tilting at a certain angle, the water droplets will roll off from the surface of the fiber felt, while gasoline will quickly penetrate into the interior of the fiber felt after contacting the surface of the polyester fiber felt.

[0047] AsFigure 4 As shown in Figure 4 , the water contact angle (WCA) of the superhydrophobic / superoleophilic polyester fiber felt is 153°( Figure 4 a), and the oil contact angle (OCA) with respect to gasoline is 0°( Figure 4 b), showing obvious superhydrophobic / superoleophilic properties.

[0048] Example 2

[0049] Step 1, prepare a superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry;

[0050] The specific process is as follows: At room temperature, zirconium butoxide is added to anhydrous methanol, and after magnetic stirring for 3 h, tetraethyl orthosilicate and dodecyltriethoxysilane are added in sequence. The molar ratio of zirconium butoxide:tetraethyl orthosilicate:dodecyltriethoxysilane is 1:2:0.1, and stirring is continued for 2 h, followed by static aging to obtain the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry. The concentration of the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry is 0.08 mol / L;

[0051] Step 2, by means of air spraying, the slurry obtained in Step 2 is sprayed onto the surface of the fiber felt. The spraying amount is such that the slurry can completely wet the surface and interior of the fiber felt. Subsequently, the slurry is evenly coated by repeated extrusion, and finally dried in an oven at 40 °C for 40 min to remove the organic solvents in the gel coating, so as to deposit the SiO 2 -ZrO 2 functional gel coating on the fiber surface of the polyester fiber felt;

[0052] Step 3, the SiO 2 -ZrO 2 functional gel coating deposited on the fiber surface of the polyester fiber felt in Step 2 is further crosslinked and cured by microwave treatment. The microwave curing power is 700 W and the curing time is 40 min to obtain a superhydrophobic / superoleophilic polyester fiber felt.

[0053] The oil absorption rates of the polyester fiber felt are as follows: 12.0 g / g for n-hexane, 13.4 g / g for gasoline, 13.0 g / g for petroleum ether, 15.3 g / g for cyclohexane, 25.8 g / g for vegetable oil, 35.2 g / g for silicone oil, 21.5 g / g for chlorobenzene, 21.8 g / g for dichloromethane, and 23.1 g / g for chloroform; the oil retention rates are as follows: 91.3 for n-hexane, 92.0 for gasoline, 91.8 for petroleum ether, 92.5 for cyclohexane, 98.3 for vegetable oil, 99.4 for silicone oil, 93.7 for chlorobenzene, 94.4 for dichloromethane, and 95.8 for chloroform. The contact angle of the modified polyester fiber felt with water is 154°, and the contact angle with vegetable oil is 0°, showing obvious superhydrophobic / superoleophilic properties.

[0054] Example 3

[0055] Step 1, prepare superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry;

[0056] The specific process is as follows: At room temperature, zirconium n-butoxide is added to anhydrous methanol, and after magnetic stirring for 5 h, tetraethyl orthosilicate and dodecyltriethoxysilane are added in sequence. The molar ratio of zirconium n-butoxide:tetraethyl orthosilicate:dodecyltriethoxysilane is 1:3:0.3. Stirring is continued for 3 h, and then it is left to age for 6 h to obtain the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry. The concentration of the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry is 0.15 mol / L;

[0057] Step 2, by means of air spraying, spray the slurry obtained in Step 2 onto the surface of the fiber felt. The spraying amount should be such that the slurry can completely wet the surface and inside of the fiber felt. Subsequently, it is evenly coated by repeated extrusion, and finally dried in an oven at 60 °C for 20 min to remove the organic solvents in the gel coating, so as to deposit the SiO 2 -ZrO 2 functional gel coating obtained in Step 1 on the fiber surface of the polyester fiber felt;

[0058] Step 3, further crosslink and cure the SiO 2 -ZrO 2 functional gel coating deposited on the fiber surface of the polyester fiber felt in Step 2 by microwave treatment. The microwave curing power is 1200 W, and the curing time is 10 min to obtain the polyester fiber felt with superhydrophobic / superoleophilic properties.

[0059] The oil absorption rates of the polyester fiber felt are as follows: 12.4 g / g for n-hexane, 13.9 g / g for gasoline, 13.6 g / g for petroleum ether, 15.5 g / g for cyclohexane, 26.2 g / g for vegetable oil, 35.4 g / g for silicone oil, 21.8 g / g for chlorobenzene, 22.3 g / g for dichloromethane, 23.7 g / g for chloroform; the oil retention rates are as follows: 91.4 for n-hexane, 92.3 for gasoline, 92.1 for petroleum ether, 92.7 for cyclohexane, 98.4 for vegetable oil, 99.5 for silicone oil, 93.8 for chlorobenzene, 94.7 for dichloromethane, 96.0 for chloroform. The superhydrophobic / superoleophilic polyester fiber felt has a water contact angle of 156° and a n-hexane contact angle of 0°, showing obvious superhydrophobic / superoleophilic properties.

[0060] Distilled water (250 mL), chlorobenzene (5 mL) and white oil emulsifier (0.1 g) were mixed and magnetically stirred for 12 h to prepare a stable milky oil-in-water (O / W) emulsion. As Figure 5 shown, a small piece of superhydrophobic / superoleophilic polyester fiber felt was cut and put into the oil-in-water emulsion. After stirring for several seconds, the oil-phase components were fully absorbed and the emulsion became clear, indicating that it has good oil-water separation performance for the oil-in-water emulsion.

[0061] The superhydrophobic / superoleophilic polyester fiber felt was immersed in 20 g / L NaCl, HCl and NaOH aqueous solutions with pH = 1 and pH = 13 for 72 h respectively. After drying, it was continued to be used for the oil-water separation of the oil-in-water emulsion. The emulsion separated by the superhydrophobic / superoleophilic polyester fiber felt was marked as fiber felt-O / W, and the emulsions separated by the superhydrophobic / superoleophilic polyester fiber felt corroded in NaCl, HCl and NaOH aqueous solutions for 72 h were marked as fiber felt NaCl -O / W, fiber felt HCl -O / W and fiber felt NaOH -O / W, as Figure 6 shown, after being corroded by 3 kinds of corrosive media, the superhydrophobic / superoleophilic polyester fiber felt still has certain oil-water separation performance for the oil-in-water emulsion.

[0062] Figure 7 For Figure 6Optical micrographs of each emulsion were used to characterize the microscopic morphology of the emulsion before and after separation. At the same time, the oil content of each emulsion after separation was measured by an ultraviolet spectrophotometer to calculate its separation efficiency for the emulsion. Before separation, the oil-in-water microdroplets were evenly and stably distributed in the emulsion, with a particle size of about 10 μm. After treatment with the superhydrophobic / superoleophilic polyester fiber felt, almost no microdroplets could be observed in the emulsion, and the separation efficiency was about 98%; after treatment with the superhydrophobic / superoleophilic polyester fiber felt corroded by NaCl and HCl solutions, only a few microdroplets with a particle size of about 1 μm were observed in the emulsion, and the separation efficiency was about 90%; after treatment with the superhydrophobic / superoleophilic polyester fiber felt corroded by NaOH solution, a few microdroplets with a particle size of about 3 μm were observed in the emulsion, and the separation efficiency was about 80%.

[0063] Example 4

[0064] Step 1, prepare superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry;

[0065] The specific process is as follows: at room temperature, zirconium butoxide is added to anhydrous methanol and anhydrous ethanol, and the mass ratio of anhydrous methanol to anhydrous ethanol is 1:1. After magnetic stirring for 6 h, tetraethyl orthosilicate and long-chain silane are added in turn. The molar ratio of zirconium butoxide:tetraethyl orthosilicate:long-chain silane is 1:4:0.5. Stir for another 4 h, and then let it stand for aging to obtain the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry, and the concentration of the superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry is 0.2 mol / L;

[0066] The long-chain silane uses dodecyltrimethoxysilane and octadecyltriethoxysilane, and the molar ratio of the two is 1:1;

[0067] Step 2, by means of air spraying, spray the slurry obtained in Step 2 onto the surface of the fiber felt. The spraying amount is based on the slurry being able to completely wet the surface and inside of the fiber felt. Then, make the slurry evenly coated by repeated extrusion. Finally, dry it in an oven at 80 °C for 5 min to remove the organic solvent in the gel coating, and the SiO 2 -ZrO 2 functional gel coating obtained in Step 1 can be deposited on the fiber surface of the polyester fiber felt;

[0068] Step 3, through microwave treatment, the SiO 2 -ZrO 2The functional gel coating is further crosslinked and cured with a microwave curing power of 1800 W and a curing time of 1 min to obtain a superhydrophobic / superoleophilic polyester fiber felt.

[0069] The oil absorption rates of the polyester fiber felt are as follows: 12.8 g / g for n-hexane, 14.3 g / g for gasoline, 14.0 g / g for petroleum ether, 15.8 g / g for cyclohexane, 26.5 g / g for vegetable oil, 35.6 g / g for silicone oil, 22.1 g / g for chlorobenzene, 22.6 g / g for dichloromethane, and 24.1 g / g for chloroform; the oil retention rates are as follows: 91.6 for n-hexane, 92.4 for gasoline, 92.2 for petroleum ether, 92.8 for cyclohexane, 98.5 for vegetable oil, 99.6 for silicone oil, 94.0 for chlorobenzene, 94.9 for dichloromethane, and 96.2 for chloroform. The contact angle of the superhydrophobic / superoleophilic polyester fiber felt with water is 160°, and the contact angle with dichloromethane is 0°, showing obvious superhydrophobic / superoleophilic properties.

[0070] Distilled water (250 mL), vegetable oil (5 mL), and emulsifier Span 80 (0.1 g) are mixed and magnetically stirred for 12 h to prepare a stable water-in-oil (W / O) emulsion. A small piece of the superhydrophobic / superoleophilic polyester fiber felt is cut and put into the water-in-oil emulsion. After stirring for a few seconds, the oil-phase components are fully absorbed, and the emulsion becomes very clear, indicating that it has better oil-water separation performance for the water-in-oil emulsion. The superhydrophobic / superoleophilic polyester fiber felt is respectively immersed in 20 g / L NaCl, HCl, and NaOH aqueous solutions with pH = 1 and pH = 13 for 72 h, and after drying, it is continued to be used for the oil-water separation of the water-in-oil emulsion. As Figure 8 shown, after being corroded by the three corrosion solutions, the superhydrophobic / superoleophilic polyester fiber felt has good oil-water separation performance for the water-in-oil emulsion.

[0071] Figure 9 For Figure 8 the optical micrographs of the emulsions, before separation, the water-in-oil microdroplets are evenly and stably distributed in the emulsion, and the particle size is about 14 μm; after separation, almost no microdroplets can be observed in each emulsion, and the separation efficiency is higher than 99.5%. It can be seen that the superhydrophobic / superoleophilic polyester fiber felt prepared by the present invention has good stability and durability, and still has good separation performance for the water-in-oil emulsion even after being corroded by acid, alkali, and salt solutions for a long time.

Claims

1. Preparation method of superhydrophobic / superoleophilic polyester fiber felt for oil-water emulsion separation, Characterized in that, It is specifically implemented according to the following steps: Step 1, prepare a superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry; The specific process of Step 1 is as follows: At room temperature, zirconium butoxide is added to an organic solvent, and after magnetic stirring for 2 h to 6 h, tetraethyl orthosilicate and a long-chain silane are added in sequence, and stirring is continued for 1 h to 4 h, and then static aging is carried out to obtain a superhydrophobic / superoleophilic SiO 2 -ZrO 2 functional slurry; The concentration of the superhydrophobic / superoleophilic SiO2-ZrO2 functional slurry is 0.01 mol / L to 0.2 mol / L, and the mass ratio of zirconium butoxide: tetraethyl orthosilicate: long-chain silane is 1:1 to 4:0.01 to 0.5; Step 2, deposit the SiO 2 -ZrO 2 functional gel coating obtained in Step 1 on the fiber surface of the polyester fiber felt by spraying treatment; Step 3, the SiO 2 -ZrO 2 functional gel coating deposited on the fiber surface of the polyester fiber felt in Step 2 is further crosslinked and cured to obtain a polyester fiber felt with superhydrophobic / superoleophilic properties.

2. The preparation method of superhydrophobic / superoleophilic polyester fiber felt for oil-water emulsion separation according to claim 1, Characterized in that, The organic solvent is one or two of absolute ethanol and absolute methanol, and the long-chain silane is one or several of dodecyltrimethoxysilane, dodecyltriethoxysilane, hexadecyltrimethoxysilane, octadecyltrimethoxysilane, and octadecyltriethoxysilane.

3. The preparation method of superhydrophobic / superoleophilic polyester fiber felt for oil-water emulsion separation according to claim 1, Characterized in that, In step 2, the spraying process is as follows: by means of air spraying, the slurry obtained in step 2 is sprayed onto the surface of the fiber felt, and then the slurry is evenly coated by repeated extrusion, and finally dried in an oven at 30°C to 80°C for 5 min to 60 min.

4. The preparation method of superhydrophobic / superoleophilic polyester fiber felt for oil-water emulsion separation according to claim 3, Characterized in that, The spraying amount is based on that the slurry can completely wet the surface and inside of the fiber felt.

5. The preparation method of superhydrophobic / superoleophilic polyester fiber felt for oil-water emulsion separation according to claim 1, Characterized in that, In step 3, the microwave curing power is 100 W to 1800 W, and the curing time is 1 min to 60 min.

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